• Title/Summary/Keyword: GC-determination

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Simultaneous Determination of Plasticizers in Food Simulants Using GC/MS

  • Park, Na-Young;Yoon, Hae-Jung;Kwak, In-Shin;Jeon, Dae-Hoon;Choi, Hyun-Chul;Eum, Mi-Ok;Kim, Hyung-Il;Sung, Jun-Hyun;Kim, So-Hee;Lee, Young-Ja
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.15 no.3
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    • pp.93-98
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    • 2009
  • Migration levels of plasticizers, di-n-butyl phthalate (DBP), benzyl-butyl phthalate (BBP), di-n-octyl phthalate(DNOP), di-iso-decyl phthalate (DIDP) and di-iso-nonyl phthalate (DINP), di-(2-ethylhexyl) adipate (DEHA), from 46 poly(vinyl chloride) (PVC) wrap films and 54 PVC gaskets into food simulants were determined using gas chromatography/mass spectrometry (GC/MS). The method was validated with limit of detection (LOD) of $0.01{\sim}0.02\;{\mu}g/mL$ for DBP, BBP, DNOP and DEHA, and $2\;{\mu}g/mL$ for DIDP and DINP. The linearity were found to be > 0.99 for all the compounds in concentration range of $0.1{\sim}81.4\;{\mu}g/mL$, and overall recoveries were ranged from 90.4 ~ 99.6%. DBP, BBP, DNOP, DEHA, DIDP and DINP were not detected in food simulants, except 1 wrap sample from which 0.28 and $0.99\;{\mu}g/mL$ of DEHA were detected respectively when tested with 20% ethanol and n-heptane as food simulants. These values were below the regulatory limitation in European Union (EU).

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Determination of Plasticizers included in Balloon by Solid Phase Microextraction and Gas Chromatography with Mass Spectrometric Detection (SPME-GC-MS를 이용하여 풍선에 포함된 가소제의 분석)

  • Park, Hyun-Mee;Kim, Ji-Hyun;Ryu, Jae-Chun;Kim, Young-Man;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.44-49
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    • 2001
  • Solid-phase microextraction (SPME) with $85{\mu}m$ polyacrylate fiber, coupled to gas chromatography-mass spectrometry was used to analyze the plasticizers contained in balloon samples. The balloons were identified to be made of polyisoprene by IR spectroscopy. The plasticizers extracted from the balloon samples soaked in acetone-added water solvent for an hour were quantified by external standard method using nine kinds of plasticizers. The quantification method was validated for standard plasticizers in the range of $0.25-25{\mu}g/g$. The detection limits were $0.11-0.38{\mu}g/g$ for different plasticizers. The RSDs for the reproducibility of this quantitation method were 3.7-14.2%. A few of balloons included risky level of plasticizer concerned as and endocrine disrupter, and it is necessary to regulate these products.

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Determination of 2, 4-D and 2, 4, 5-T in River Water and Drinking Water by Gas Chromatograph/Mass Spectrometer (GC/MS를 이용한 수질시료 중 2, 4-D와 2, 4, 5-T의 분석에 관한 연구)

  • 표희수;신혜승;박송자
    • Environmental Analysis Health and Toxicology
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    • v.15 no.3
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    • pp.107-113
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    • 2000
  • Chlorophenoxy acids are one of the most useful classes of chlorinated herbicides. Specially 2, 4-D and 2, 4, 5-T were known to endocrine distruptors. In this study, these pesticides in water samples were extracted by liquid-liquid extration at acidic conditions and then derivatization of acidic group was carried out various esterifications using by CH$_3$I/Acetone -K$_2$CO$_3$, H$_2$SO$_4$/MeOH or TFAA/TFE. That result, Sensitivities of TFE derivatized 2, 4-D and 2, 4, 5-T are prior to the others. The recoveries of 2, 4-D and 2, 4, 5-T were 98% and 82% respectively using diethyl ether as an extracting solvent.

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Simultaneous Determination of Cannabidiol, Cannabinol, and ${\Delta}^9-Tetrahydrocannabinol$ in Human Hair by Gas Chromatography-Mass Spectrometry

  • Kim Jin Young;Suh Sung Ill;In Moon Kyo;Paeng Ki-Jung;Chung Bong Chul
    • Archives of Pharmacal Research
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    • v.28 no.9
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    • pp.1086-1091
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    • 2005
  • An analytical method was developed for evaluating the cannabidiol (CBO), cannabinol (CBN), ${\Delta}^9-tetrahydrocannabinol$ $({\Delta}^9-THC)$ level in human hair using gas chromatography-mass spectrometry (GC-MS). Hair samples (50mg) were washed with isopropyl alcohol and cut into small fragments (< 1mm). After adding a deuterated internal standard, the hair samples were incubated in 1.0M NaOH for 10 min at $95^{\circ}C$. The analytes from the resulting hydrolyzed samples were extracted using a mixture of n-hexane-ethyl acetate (75:25, v/v). The extracts were then evaporated, derivatized, and injected into the GC-MS. The recovery ranges of CBD, CBN, and ${\Delta}^9-THC$ at three concentration levels were $37.9-94.5\%$ with good correlation coefficients $(r^2>0.9989)$. The intra-day precision and accuracy ranged from $-9.4\%\;to\;17.7\%$, and the inter-day precision and accuracy ranged from $-15.5\%\;to\;14.5\%$, respectively. The limits of detection (LOD) for CBD, CBN, and ${\Delta}^9-THC$ were 0.005, 0.002, and 0.006 ng/mg, respectively. The applicability of this method of analyzing the hair samples from cannabis abusers was demonstrated.

Determination of pesticides in dead wild birds in Korea (우리나라 폐사 야생조류에서의 농약 분석)

  • Kim, MeeKyung;Yun, Seon Jong;Kim, Dong-Gyu;Bong, Young-Hoon;Kim, Heuijin;Jang, Jung-Hee;Chung, Gab-Soo
    • Korean Journal of Veterinary Research
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    • v.48 no.2
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    • pp.131-137
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    • 2008
  • Pesticides are extensively used for the control of crop pests in agriculture and forestry. Organophosphate (OP) and carbamate pesticides are especially effective for the control of a variety of harmful insects. However, these cholinesterase inhibitors are also dangerous to non-target organisms (wildlife and other animals) because of their high acute toxicity. Most poisonings by pesticides occur as a result of misuse or accidental exposure, but intentional killing of unwanted animals also occurs. At the request of a local autonomous entity, we investigated wild bird poisonings by pesticides from 2003 to 2007. The 207 suspicious samples of pesticide poisoning based on the necropsy were analyzed by GC/NPD, GC/FPD, or GC/MSD. We looked for trends in the identification of pesticides in wild birds thought to have died from poisoning. Pesticides were determined in 59% of the total samples analyzed. Phosphamidon and monochrotophos were the most common pesticides identified, which amounted to 77% of the subtotal. Other OP and carbamate pesticides were also found in various concentrations from dead wild birds. The determined rates of pesticides were as high as 86% and 76% in 2003 and 2006, respectively, during an outbreak of avian influenza in Korea.

Determination of Phthalic Acid Esters and Adipate in Sediment Samples (저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Yoon, Sung-Ho;Cho, Hyun-Woo;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.360-364
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    • 2002
  • The most common 8 phthalic acid esters (PAEs) and adipate in sediment were measured 5 times from 1999 to 2001 at 11 sites of river in Korea. Ultrasonication extraction with dichloromethane was done for extraction of the sediment. After concentration GC/MS-SIM analysis was performed. Three compounds (DEP, DBP and DEHP) among eight phthalic acid esters were detected from the sediment samples, and the other PAEs were not detected in any samples. DEHP (27.3~63.6%) was detected with higher frequency than any other compounds for sediment samples. And this compound had shown the highest average concentration (81.7~427.6 ng/g).

Quantitative Approaches for the Determination of Volatile Organic Compounds (VOC) and Its Performance Assessment in Terms of Solvent Types and the Related Matrix Effects

  • Ullah, Md. Ahsan;Kim, Ki-Hyun;Szulejko, Jan E.;Choi, Dal Woong
    • Asian Journal of Atmospheric Environment
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    • v.11 no.1
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    • pp.1-14
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    • 2017
  • For the quantitative analysis of volatile organic compounds (VOC), the use of a proper solvent is crucial to reduce the chance of biased results or effect of interference either in direct analysis by a gas chromatograph (GC) or with thermal desorption analysis due to matrix effects, e.g., the existence of a broad solvent peak tailing that overlaps early eluters. In this work, the relative performance of different solvents has been evaluated using standards containing 19 VOCs in three different solvents (methanol, pentane, and hexane). Comparison of the response factor of the detected VOCs confirms their means for methanol and hexane higher than that of pentane by 84% and 27%, respectively. In light of the solvent vapor pressure at the initial GC column temperature ($35^{\circ}C$), the enhanced sensitivity in methanol suggests the potential role of solvent vapor expansion in the hot injector (split ON) which leads to solvent trapping on the column. In contrast, if the recurrent relationships between homologues were evaluated using an effective carbon number (ECN) additivity approach, the comparability assessed in terms of percent difference improved on the order of methanol (26.5%), hexane (6.73%), and pentane (5.24%). As such, the relative performance of GC can be affected considerably in the direct injection-based analysis of VOC due to the selection of solvent.

The Extraction and Derivatization of Organotins in Water Sample by Gas Chromatograph/Mass Spectrometer (기체크로마토그래프/질량분석기에 의한 물시료 중 Organotin의 추출 및 유도체 반응에 관한 연구)

  • Hong, Jee-Eun;Lee, Kang-Jin;Pyo, Hee Soo;Park, Song-Ja;Lee, Won
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.636-645
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    • 2000
  • A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

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Determination of Phthalate Esters and Adipate in Water and Sediment Samples (수질 및 저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.616-623
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    • 2000
  • The most common phthalate acid esters (8 compounds) and adipate were determined from water and sediment simultaneously. After liquid-liquid extraction with n-hexane for water and sonication extraction with dichloromethane for sediment, these were determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.993$) on the range of the 0.1-20 ng/ml (water) and 10-500 ng/g (sediment), and the detection limits of method were below 0.1 ng/ml and 10 ng/g for water samples and sediment samples, respectively. The method shows a good precision and accuracy for measurement of phthalates and adipate.

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Volatile organic compounds of pyroligneous liquor of bamboo sprout produced in damyang-gun (담양군 죽초액의 휘발성성분 분석)

  • Lee, Eunsil;Jang, Hyejin;Lee, Songjin;Ha, Jaeho
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.299-306
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    • 2013
  • Pyroligneous liquor as a byproduct from charcoal production of bamboo sprout produced damyang-gun has the broad benefits such as improvement of soil quality, plant growth control and is mainly used for the treatment of atopic dermatitis, fungi and many other skin diseases. In this study, flavor compounds of pyroligneous liquor from bamboo sprout produced in Damyang-gun were analyzed and compared using three different methods including direct analysis (DA), headspace solid phase microextraction (HS-SPME) and stir bar sorptive extraction (SBSE). Simultaneously, the analytical conditions of GC-MS for the determination of volatile compounds were optimized. Based on volatile organic compounds detected by GC-MS, SBSE and SPME methods showed higher sensitivity than direct analysis. Major compounds of pyroligneous liquor were cresol, guaiacol, p-ethyl guaiacol and syringol. These phenolic compounds are reported as the useful chemicals with medicinal activity.